High pressure apparatus



y 1964 R. H. WENTORF, JR ,1

HIGH PRESSURE APPARATUS Filed Feb. 28. 1961 /nvemar: Robe/'2 H, Wenforf,Jr,

United States Patent Q 3,134,139 HIGH PRESSURE APPARATUS Robert H.Wentorf, Jr., Schenectady, N.Y., assignor to v General Electric Company,a corporation of New York Filed Feb. 28,1961, Ser. No. 92,341

2 Claims. {131. 18-16) This invention relates to an improved highpressure high temperature apparatus, more particularly, to a highpressure high temperature apparatus of the multiple punch type withimproved high strength pressure resisting members together with improvedlateral support for the punches.

Previous multiple punch high pressure high temperature apparatusesemploy a plurality of punches which move along a predetermined linetowards a central point to define a reaction chamber in which a specimenmaterial is placed to be subjected to high pressures and hightemperatures. These plural punch apparatuses generally include puncheswhose configurations are usually trapezoidal and which interfit todefine a central reaction chamber. A suitable example of such a multiplepunch apparatus is disclosed in copending application Serial No.855,867-Bundy, filed November 27, 1959, now Patent No. 3,107,395 andassigned to the same assignee as the present invention. In theaforementioned application 6 or more inwardly directed and interfittingtrape- "at a minimum for proper alignment and other operating purposes,so that the lesser the number of punches that need be moved, the moreefiicient the apparatus. These multiple punch apparatuses also includeprovision for gasketing between all mating punch surfaces, and motion ofthe punches occurs together with compression of the gasketin-g.Accordingly, a considerable amount of press force is lost because it isnecessary to compress the gaskets, so that an apparatus with minimumamounts of gasketing is also more desirable.

Accordingly, it is an object of this invention to provide an improvedhigh pressure high temperature apparatus.

It is another object of this invention to provide an improved highpressure high temperature multiple punch apparatus with fewer than allpunches being moved to provide pressure in a specimen material.

It is a further object of this invention to minimize gasketing in amultiple punch apparatus.

=I-t is yet another object of this invention to provide multiple punchapparatus where vertical anvils are used in combination with lateralpunches.

It is another object of this invention to provide improved lateralsupport means for multiple punches.

Briefly described, this invention in one form includes a pair of wide,massive anvil members with opposed substantially flat faces which arespaced apart, and a plurality of lateral punches moving radiallyinwardly between the said flat faced anvil members to define a reactionvolume in which a specimen material is placed to be subjected to highpressures and high temperatures.

This invention will be better understood when taken in connection withthe following description and the drawing in which:

FIG. 1 is a partial elevation and cross sectional view of a preferredform of this invention;

FIG. 2 is a partial and top view of FIG. 1 taken on the FIG. 3 is amodification of the invention illustrated in FIG. 1 with respect to thelateral punches; and

FIG. 4 is a partial cross sectional top View of FIG. 3 illustrating thearrangement and gasketing of the lateral punches.

Referring now to FIG. 1, there is illustrated a preferred form of a highpressure high temperature apparatus 10 :which includes essentially apair of oppositely directed and spaced apart massive anvil members illand 12 and a plurality of lateral punches 13 and 14- (FIG. 1), and 15and 16 (FIG. 2). Anvil members 11 and 12 and punches 13 through 16define a reaction volume 17 in which a specimen material, or a reactionvessel containing a specimen material, may be subjected to highpressures and high temperatures. 'Because anvil members 11 and 12 aremade very massive and large, and because their opposed faces 18 aregenerally fiat, they inherently possess very high strength and areextremely resistant to fracture at high pressures and temperatures.While these anvils may be of a one piece. material, such as for example,high grade steel, it is, however, contemplated that they may comprise aplurality of press fitted or shrunk fitted rings about a central hardblock of,.for example, Carboloy cemented carbide, as indicated in US.Patent 2,941,248- Hall. Anvils 11 and 12 are positioned oppositely toeach other and are adapted to be moved towards each other althoughmovement of these punches to compress a specimen in chamber 17 is notnecessary. These anvils do not interfit to provide a reaction chamberand thus may be manufactured in the wide fiat configuration, asdisclosed, with inherent high lateral support and strengthcharacteristics. Because of the high strength characteristics, theparticular structure and the arrangement of parts as illustrated in FIG.1, anvils 11 and 12 may merely be vertically adjustable to provide adesired spacing therebetween or adjustable for various pressures with inthe reaction volume. A simple means of adjusting anvils 11 and 12.include, a piston and cylinder arrangernent 19, as illustrated in FIG.1, with a hydraulic cylinder 2i and piston 21. Anvil 11 (and similarlyanvil 12) is made separate from piston 21 and suitably attached theretoto facilitate assembly, disassembly, and replacement. Hydraulic orpneumatic fluid under pressure enters cylinder 20 by means of conduit 22to move anvil members 11 and 12 towards each other. It is, however,contemplated that various mechanical means may also be utilized toadjust and move the anvil members 11 and 12 because they are notemployed primarily to compress a specimen material in volume 17.

Positioned between and radially within the spaced apart anvil members 11and 12 and laterally thereof are the prism like extremities of aplurality of lateral punches 1'3 and 14 (FIG. 1) and 1-5 and 16 (FIG.2). It is under stood that 2, 3, 4, 5, or more lateral punches may beemployed, however, in a preferred form of this invention fourcircumferentially spaced lateral punches 13 through 16 are employed.Each punch, for example punch 13, comprises a base 23 and straight shankportion 24 the latter having its prism-like extremity with the upper andlower bases thereof of trapezoidal shape as seen in FIG. 2. Lateralpunches 13 through 16 are adapted to be moved towards each other tocompress a specimen in reaction Volume 17. Means to provide the requiredmotion include individual or interconnected hydraulic cylinders 25together with pitsons 26 to which the lateral punches are attached. Asuitable pressure fluid is introduced into cylinder 25 by means ofconduit 27 to move the lateral punches towards each other.

FIG. 2 illustrates a top view of the lateral punches 13 through '16.Punches 13 through 16 may be described as having a cross sectionaltrapezoidal configuration, or alternatively, are tapered towards oneend. These punches 13 through 16 are positioned equidistantly incircumferential relationship to provide a substantially closed reactionvolume 17. Each punch is also in interfittin'g relationship with, orbetween, adjacent punches for support purposes. In accordance with US.Patent 2,94l,248-Hall, and copending application Serial No. 855,867Bundy, suitable gasketing 27 is provided between each lateral punch, notonly to provide static sealing of the reaction volume 17, or a reactionvessel therein, but also to provide motion of the lateral punchessimultaneously with compression of the gaskets so that a specimenmaterial in reaction volume 17 may be suitably compressed. Variousmaterials may be used for gasketing 27. Examples of preferred materials,include pyrophyllite, catlinite, talc and other such ceramic andstone-like materials. Alternatively, however, gasketing may be providedby extrusion of an oversize reaction vessel material, or specimenmaterial within the reaction volume 17, into the intervening spacesbetween punches 13 through 16. It is an important criteria of gasketingthat sufiicient gas-keting be employed between adjacent punches 12 toprovide the required lateral support so that each punch 12 may in turnsupport an adjacent punch for a high strength apparatus. Accordingly,depending on the size of the apparatus, gasketing should extend on theorder of one-half to several widths of a lateral punch face 28,extending radially outward from the reaction volume 17. However, caremust be taken not to employ too much gasketing because compression oftoo much gasketing will limit radially inward punch motion or strokeavailable, or limit the pressure that can be reached in the reactionvessel since too much applied punch force will be employed to compressthe gaskets and not enough force will remain to attain high pressure inthe specimen in volume 17. Referring again to FIG. 1, one of theadvantages of this invention is the elimination of the type of gasketingdescribed, bet-ween surfaces 18 of anvils 11 and 12 and lateral punches13 through 16. In order to provide relative freedom for radially inwardmotion of lateral punches 13 through 16 with respect to anvil members 11and 12, a suitable medium 29 in the form of a lubricant and/or gasketmaterial is employed. A coefficient of friction of .0 5 or lower may bereached between highly loaded surfaces such as between punches 13through 16 and anvils 11 and 12 by use of proper lubricants, forexample, MoS castor oil, Teflon, soft metals, AgC l, etc. Additionally,that portion '24 of lateral punches 13 through 16 may include a veryslight taper (not shown) converging towards the inner face portion orvolume 17 to retain light forms of gasketing. Either pontions 24 oflateral punches 13 through 16 or the anvils 11 and 12, or both, may besuitably (slightly) tapered to provide this type of gasketing, sealing,or lubricating means. It is to be understood, however, that a taper onthe order of 5 may be employed, which, in conjunction with a large flatanvil member, does not weaken the members. Such tapering also may act asa compensation for distortions of the apparatus under high loadingconditions. Medium 29 is not, however, primarily a gasket becausesealing at this position is a relatively simple matter where motionacross a very narrow space is non-existent or extremely limited.Lubrication is far more important than sealing here.

Motion of lateral punches may be limited to less than all of the punchesand yet provide high pressure subjection of the reaction vessel. Forexample, in FIG. 2, upper punch 15 may be stationary while punches 13and 14 may be moved towards punch 15. In this manner only motion ofpunch 16 is required to compress a specimen in volume 17. By the sametoken, it is understood also that only two punches may move, and, bysimilar arrangement, any number of punches may be moved. It is, ofcourse, obvious that reaction volume 17 may have various configurationsboth geometrical and irregular, such as, cubic, rectangularparallelepiped, and various other plural sided figures both curvedand/or 41 linear. The specific configuration of reaction volume 17depends on the shape of the faces of punches 13 through 16 and on thenumber of such punches employed.

An electrical circuit is established to heat a specimen in volume 17 byresistance heating. In FIG. 1, electrical conductors 3i) and 31 areconnected to, for example, anvils 11 and 12, respectively, and to asource of power (not shown). Punches 13 through 16 are electricallyinsulated from anvils 11 and 12 preferably by means of lubricant orgasket 28, as described. Reaction volume 17 may contain an electricalresistance heater, a reaction vessel incorporating electrical circuitry,or the specimen itself be or made electrically conductive. An electricalcircuit is thus established between anvils 11 and 12 and throughreaction volume 17. Reference is made, in this respect, to theaforementioned Hall patent and copending Bundy application.

In an exemplary operation of this invention, anvils 11 and 12 arewithdrawn or adjustably spaced vertically, and punches 13 through iswithdrawn radially outward so that described gasketing 27 may bepositioned between punches and anvils if gasketing is not provided byextrusion. Thereafter, a specimen or reaction vessel is positioned involume 17 and the lateral punches 13 through 16 and anvils 11 and 12brought together snugly with, of course, a lubricant gasket 29 betweenthe punches and the anvils. From this point, high pressure is generatedin reaction volume 17 by inward motion of one or more of the lateralpunches 13 through 16 with anvils 11 and 12 being adjusted to maintainthe pressure. Alternatively, anvils 11 and 12 may be preadjusted tomaintain these pressures or may have some motion towards or away fromeach other at the same time punches 13 through 16 move. It is animportant feature of this invention that anvils 11 and 12 are notordinarily required to be movable in the same sense as those punches ofthe aforementioned Hall patent or Bundy application. In essence, anvils11 and 12 define a pair of very strong platelike surfaces describing ahollow disc-like volume in which punches 13 through 16 slide.

A modification of the invention of FIG. 1 is shown in FIG. 3. Referringnow to FIG. 3, the apparatus of FIG. 1 is modified so that at least oneand preferably both opposed flat faced anvils 32 and 33 contain ashallow frustoconical depression 34 therein. Within depression 34 aplurality of, for example, 4 lateral punches 35 and 36 (FIG. 3), and 37and 38 (FIG. 4) are positioned. These punches 35 through 38 converginglytaper from their innermost ends or faces 39 to their outermost end 40 toprovide a shallow trapezoidal cross sectional configuration. The taperof depression 34 and avils 32 and 33 coincides with the taper of thefrustoconical cross sectional configuration of punches 35 through 38.When lateral punches 35 through 38 are placed in depression 34 asillustrated, and anvil members 32 and 33 are caused to move together,punches 35 through 38 are also caused to slide inwardly to compress aspecimen material, or reaction vessel containing a specimen material, involume 17.

FIG. 4 is a top and sectional view of FIG. 3 illustrating four lateralpunches 35 through 38 residing within a depression 34. Gasketing 27 maybe employed between the lateral punches 35 through 38 much in the samemanner as gasketing 27 is employed as disclosed in FIG. 2. Depression 34is shallow enough so as not to weaken anvil members 32 and 33 but isdeep enough to provide inward motion of the lateral punches 35 through38 without excessive force on the anvil members. An angle of about 10 to20 provides proper distribution of forces for satisfactory operation. Itis understood that movement of anvils 32 and 33 as anvils 11 and 12 islimited and that they act primarily as force blocks. The taper ofpunches 35 through 38 with corresponding depression 34 taper is usedprimarily for punch sliding purposes and not primarily to provide motionof anvils 32 and 33 with compression of gasketing as in interfittingmultiple punch apparatus. Also, because the anvils posses high strengthin the illustrated configuration, they are not in need of lateralsupport such as by adjacent punches.

It can thus be seen that this invention provides a high pressure hightemperature apparatus having a minimum number of parts which requireextensive motion and a maximum number of parts which are of massiveshape and hence of high inherent strength to thus be resistant tobreakage. There is also provided an improved sealing and gasketingarrangement which overcomes the disadvantages of too much gasketing withinherent stroke and sealing problems. In some instances lubrication maybe dispensed with between the punches and the anvils depending on themode of adjustment of parts during operation, the material and finish ofthe parts. Lubrication is a preferred form of the invention.

Accordingly, while specific apparatuses have been described and shown,it is not intended that they be limited to this invention and it iscontemplated that all modifications known to those skilled in the art beincluded herewith as indicated in the scope of the appended claims.

What I claim as new and desire to secure by Letters 7 Patent of theUnited States is:

l. A high pressure, high temperature apparatus comprising incombination:

(a) a pair of massive anvil members each having an extensivesubstantially fiat face;

(1) said faces being in apposition to each other in substantiallyparallel spaced relation;

(b) at least three punches having substantially identical prism-likeextremities extending into the space between said faces;

(1) said extremities each having a first and a second flat side mutuallyparallel and trapezoidallyshaped, a relatively small front fiat punchface at the distal end of the extremity and two flat rectangular sideportions converging inwardly of said space to meet said punch face;

(2) said extremities being disposed between said anvil members havingall said first fiat sides contiguous with and slidably engaging one ofthe flat anvil faces, having all said second flat sides contiguous withand slidably engaging the other of the flat anvil faces and having eachconverging rectangular side portion of each extremity located adjacentto and substantially coextensive with a converging rectangular sideportion of another extremity;

(c) sealing means disposed between said adjacent rectangular sideportions;

(1) said punch faces, sealing means and flat anvil faces cooperating todefine a centrally-located closed reaction volume;

(d) means for providing relative movement between said anvil members tofixedly space said anvil members in slidable contact with said first andsecond flat sides, and

(e) means for laterally sliding at least one of said extremitiesradially inwardly of said space relative to said fixed fiat anvil faces,

whereby said sealing means are compressed and a specimen of materialcontained in said reaction volume is subjected to high active lateralforce application and high passive resistance at 90 to the active forceapplication.

2. A high pressure, high temperature apparatus comprising incombination:

(a) a pair of massive anvil members each having an extensivesubstantially flat face;

(1) said faces being in apposition to each other in substantiallyparallel spaced relation;

(b) at least three punches having substantially identical prism-likeextremities extending into the space between said faces;

(1) said extremities each having a first and a second flat side mutuallyparallel and trapezoidally-shaped, a relatively small front flat punchface at the distal end of the extremity and two flat rectangular sideportions converging inwardly of said space to meet said punch face;

(2) said extremities being disposed between said anvil members havingall said first flat sides contiguous with one of the flat anvil faces,having all said second fiat sides contiguous with the other of the fiatanvil faces and having such converging rectangular side portion of eachextremity located adjacent to and substantially co extensive with aconverging rectangular side portion of another extremity;

(c) a layer of lubricant disposed between said flat anvil faces and thefirst and second flat sides of said extremities;

(1) said lubricant being adapted to reduce the coefficient of frictiontherebetween to 0.05 or lower;

(d) sealing means disposed between said adjacent rectangular sideportions;

(1) said punch faces, sealing means and flat anvil faces defining acentrally-located closed reaction volume;

(2) means for providing relative movement between said anvil members tofixedly space said anvil members in slidable contact with said first andsecond flat sides, and

(1) means for laterally sliding at least one of said extremitiesradially inwardly of said space relative to said fixed flat anvil faces,

whereby said sealing means are compressed and a specimen of materialcontained in said reaction volume is subjected to high active lateralforce application and high passive resistance at to the active forceapplication.

References Cited in the file of this patent UNITED STATES PATENTS574,404 Du Brul Jan. 5, 1897 588,938 Albrecht et al Aug. 31, 1897921,489 Webb May 11, 1909 1,352,160 Willard Sept. 7, 1920 2,043,366 Bech.Tune 9, 1936 2,125,068 Dempsey July 26, 1938 2,941,244 Wentorf June 21,1960 2,968,837 Zeitlin et al. Jan. 24, 1961 3,044,113 Gerard et al July17, 1962 3,061,877 Custers et al. Nov. 6, 1962 3,088,168 Lloyd et al.May 7, 1963 FOREIGN PATENTS 681,847 France Feb. 4, 1930 820,327 GreatBritain Sept. 16, 1959

1. A HIGH PRESSURE, HIGH TEMPERATURE APPARATUS COMPRISING INCOMBINATION: (A) A PAIR OF MASSIVE ANVIL MEMBERS EACH HAVING ANEXTENSIVE SUBSTANTIALLY FLAT FACE; (1) SAID FACES BEING IN APPOSITION TOEACH OTHER IN SUBSTANTIALLY PARALLEL SPACED RELATION: (B) AT LEAST THREEPUNCHES HAVING SUBSTANTIALLY IDENTICAL PRISM-LIKE EXTREMITIES EXTENDINGINTO THE SPACE BETWEEN SAID FACES: (1) SAID EXTREMITIES EACH HAVING AFIRST AND A SECOND FLAT SIDE MUTUALLY LPARALLEL AND TRAPEZOIDALLYSHAPED,A RELATIVEL SMALL FRONT FLAT PUNCH FACE AT THE DISTAL END OF THEEXTREMITY AND TWO FLAT RECTANGULAR SIDE PORTIONS CONVERGING INWARDLY OFSAID SPACE TO MEET SAID PUNCH FACE; (2) SAID EXTREMITIES BEING DISPOSEDBETWEEN SAID ANVIL MEMBERS HAVING ALL SAID FIRST FLAT SIDES CONTIGUOUSWITH AND SLIDABLY ENGAGING ONE OF THE FLAT ANVIL FACES, HAVING ALL SAIDSECOND FLAT SIDES CONTIGUOUS WITH AND SLIDABLY ENGAGING THE OTHER OF THEFLAT ANVIL FACES AND HAVING EACH CONVERGING RECTANGULAR SIDE PORTION OFEACH EXTREMITY LOCATED ADJACENT TO AND SUBSTANTIALLY COEXTENSIVE WITH ACONVERGING RECTANGULAR SIDE PORTION OF ANOTHER EXTREMITY; (C) SEALINGMEANS DISPOSED BETWEEN SAID ADJACENT RECTANGULAR SIDE PORTIONS; (1) SAIDPUNCH FACES, SEALING MEANS AND FLAT ANVIL FACES COOPERATING TO DEFINE ACENTRALLY-LOCATED CLOSED REACTION VOLUME; (D) MEANS FOR PROVIDINGRELATIVE MOVEMENT BETWEEN SAID ANVIL MEMBERS TO FIXEDLY SPACE SAID ANVILMEMBERS IN SLIDABLE CONTACT WITH SID FIRST AND SECOND FLAT SIDES, AND(E) MEANS FOR ALATERALLY SLIDING AT LEAST ONE OF SAID EXTREMITIESRADIALLY INWARDLY OF SAID SPACE RELATIVE TO SAID FIXED FLAT ANVIL FACES,WHEREBY SAID SEALING MEANS ARE COMPRESSED AND A SPECMEN OF MATERIALCONTAINED IN SAID REACTION VOLUME IS SUBJECTED TO HIGH ACTIVE LATERALFORCE APPLICATION AND HIGH PASSIVE RESISTANCE AT 90* TO THE ACTIVE FORCEAPPLICATION.